HRID5720
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To 314 mg of the amorphous compound obtained in Example 9, were added 2 ml of 1,2-ethanedithiol and 1 ml of boron trifluoride/ethyl ether, and the mixture was stirred at a room temperature for 18 hours. After the addition of saturated sodium bicarbonate aqueous solution, the reaction mixture was extracted twice with a mixture of chloroform and methanol (1:1), and the extract was dried over magnesium sulfate and concentrated under a reduced pressure to obtain a residue, which was then applied to a silica gel column and eluted with chloroform/methanol (50:1 to 20:1) to obtain 213 mg of the title compound in a colorless amorphous form.
WORKUP
后处理
- extractionthe reaction mixture was extracted twice with a mixture of chloroform and methanol (1:1)
- dry with materialthe extract was dried over magnesium sulfate
- concentrationconcentrated under a reduced pressure
- customto obtain a residue, which
- washeluted with chloroform/methanol (50:1 to 20:1)